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3-环己基丙酸的合成
引用本文:宁春利,冯世强,张春雷.3-环己基丙酸的合成[J].精细化工中间体,2011,41(5):41-44.
作者姓名:宁春利  冯世强  张春雷
作者单位:1. 上海华谊集团技术研究院,上海,200241
2. 上海华谊丙烯酸有限公司,上海,200137
摘    要:以丙烯酸甲酯和环己醇为原料,经过酯交换反应合成γ,γ-环戊基丁内酯,γ,γ-环戊基丁内酯加氢得到3-环己基丙酸。考察了2步反应的催化剂和反应条件对产物收率的影响。研究结果表明,酯交换反应的优化条件为:过氧化二叔丁基为引发剂,n(丙烯酸甲酯)∶n(环己醇)=1∶4,反应温度160℃,反应时间6 h;在该条件下,γ,γ-环戊基丁内酯的收率可达93.3%;以0.5%铅/氧化铝为催化剂,γ,γ-环戊基丁内酯加氢反应的优化条件为:反应温度为250℃,γ,γ-环戊基丁内酯空速0.2 h-1,反应压力3.0 MPa,氢气空速500 h-1,在该条件下,γ,γ-环戊基丁内酯转化率78.0%,环己基丙酸选择性80.2%。

关 键 词:3-环己基丙酸  菠萝酯  丙烯酸甲酯  环己醇  γ  γ-环戊基丁内酯

Synthesis of 3-Cyclohexylpropionic Acid
NING Chun-li,FENG Shi-qiang,ZHANG Chun-lei.Synthesis of 3-Cyclohexylpropionic Acid[J].Fine Chemical Intermediates,2011,41(5):41-44.
Authors:NING Chun-li  FENG Shi-qiang  ZHANG Chun-lei
Affiliation:NING Chun-li1,FENG Shi-qiang2,ZHANG Chun-lei1(1.Technology Research Institute of Shanghai Huayi Group,Shanghai 200241,China,2.Shanghai Huayi Acrylic Acid Co.,Ltd.,Shanghai 200137,China)
Abstract:3-Cyclohexylpropionic acid was prepared by hydrogenation of γ,γ-cyclopentyl butyrolactone,which was synthesized by transesterification of methyl acrylate and cyclohexanol.The influences of catalyst and reaction conditions have been studied.The optimum conditions for the transesterification include the temperature of 160℃,the molar ratio of methyl acrylate to cyclohexanol of 1 to 4,the reaction time of 6 hours and di-tert-butyl peroxide as the initiator.Over the catalyst of 0.5%Pd/Al2O3,the conversion of γ,γ-cyclopentyl butyrolactone and the selectivity of 3-cyclohexylpropionic acid can reach 78.0% and 80.2%,respectively,under the optimum condition of 250℃,3.0 MPa,LHSV of γ,γ-cyclopentyl butyrolactone of 0.2 h-1 and GHSV of H2 of 500 h-1.
Keywords:3-cyclohexylpropionic acid  pineapple ester  methyl acrylate  cyclohexanol  γ  γ-cyclopentyl butyrolactone
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